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Pentaphosphaferrocenes [Cp R Fe(η 5 ‐P 5 )] ( 1 ) and Cu I  halides are excellent building blocks for the formation of discrete supramolecules. Herein, we demonstrate the potential of Cu(CF 3 SO 3 ) for the construction of the novel 2D polymer [{Cp*Fe(μ 4 ,η 5:1:1:1 ‐P 5 )}{Cu(CF 3 SO 3 )}] n  ( 2 ) and the unprecedented nanosphere (CH 2 Cl 2 ) 1.4 @[{Cp Bn Fe(η 5 ‐P 5 )} 12 {Cu(CF 3 SO 3 )} 19.6 ] ( 3 ). The supramolecule  3  has a unique scaffold beyond the fullerene topology, with 20 copper atoms statistically distributed over the 30 vertices of an icosidodecahedron. Combinatorics was used to interpret the average disordered structure of the supramolecules. In this case, only two pairs of enantiomers with D 5  and D 2  symmetry are possible for bidentate bridging coordination of the triflate ligands. DFT calculations showed that differences in the energies of the isomers are negligible. The benzyl ligands enhance the solubility of  3 , enabling NMR‐spectroscopic and mass‐spectrometric investigations.

An Icosidodecahedral Supramolecule Based on Pentaphosphaferrocene: From a Disordered Average Structure to Individual Isomers